CN106018646A - Non-directional screening method for azopigment in chilli sauce - Google Patents

Non-directional screening method for azopigment in chilli sauce Download PDF

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CN106018646A
CN106018646A CN201610530511.3A CN201610530511A CN106018646A CN 106018646 A CN106018646 A CN 106018646A CN 201610530511 A CN201610530511 A CN 201610530511A CN 106018646 A CN106018646 A CN 106018646A
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azopigment
ion
mass
sample
detection
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CN106018646B (en
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王骏
祝建华
胡梅
宿书芳
薛霞
刘艳明
徐大玮
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Shandong Institute for Food and Drug Control
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Shandong Institute for Food and Drug Control
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/14—Preparation by elimination of some components
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/14—Preparation by elimination of some components
    • G01N2030/146—Preparation by elimination of some components using membranes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds

Abstract

The invention relates to a non-directional screening method for azopigment in chilli sauce, and belongs to the technical field of food detection. The method comprises the steps that detection is conducted by adopting a liquid chromatography-quadrupole mass spectrometer with an electrospray ionization source, precursor ion scanning detection is conducted by taking m/z156 as daughter ions, and azopigment screening is conducted through the mass-to-charge ratio of precursor ions corresponding to chromatographic peaks in a mass chromatogram; if a total ion chromatogram containing the daughter ions 156 is obtained, it shows that a test sample contains the azopigment; the mass numbers of parent ions corresponding to the chromatographic peaks in the total ion chromatogram are checked one by one, and then forbidden or restricted pigments contained in the sample can be determined by contrasting a possible azopigment list. According to the method, when detection is conducted, no standard substance is needed for contrasting, a professional screening database does not need to be established through the standard substances, therefore, the detection cost is significantly reduced, and detection is not limited by the conditions that the standard substances are lacked, and no professional database exists; sample pretreatment only needs 20 min, instrumental analysis needs 15 min, and the single sample non-directional screening whole process only needs 35 min.

Description

The non-directional screening method of azopigment in a kind of Fructus Capsici sauce
Technical field
The present invention relates to the non-directional screening method of azopigment in Fructus Capsici sauce, belong to technical field of food detection.
Background technology
1, azopigment brief introduction
Azopigment is the pigment prepared with chemical synthesis process, and itself is without any nutritive value.Compared with natural pigment, Azopigment more can increase food appearance aesthetic feeling and can promote desire to buy and the appetite of people, and cheap, and color is beautiful, property Matter is stable, and color matching facilitates soluble, easily mixes colours, is widely used to food industry, particularly the food such as Fructus Capsici sauce, in order to pursue Beautiful in colour and lasting, Producer would generally add synthetic dyestuff.The azopigment used is allowed mainly to have carmine, Herba Amaranthi tricoloris at present Dish is red, sunset yellow, lemon yellow etc., and in GB2760 " food additive use sanitary standard ", these pigments of strict regulations is suitable for Scope and consumption.But, belong to the acid orange of azopigment, Indian yellow, Sudan red, Sudan II, red Ⅲ, tonyred together IV etc. forbids adding in food.
These forbid add azopigment many with aromatic hydrocarbons chemical products such as benzene, toluene, naphthalenes as raw material, through sulfonation, A series of organic reaction such as nitrification, azo is bound up.They through bioconversion, can form carcinogen in human body.When , there are some illegal retailers in front society because keeping out the temptation of incessantly profit, some cheap works of illegal interpolation in the food produced Industry pigment.In February, 2005, Something English office is found to have 350 numerous food and is polluted by " Sudan red 1 number ", it is simply that abuse The typical case of industry azopigment.After tonyred, several azopigments are had again to be found in the food such as Fructus Capsici sauce, Such as para red, rhodamine B etc..The phenomenon of this type of illegal interpolation occurs the most again and again, is on the one hand the chilli products such as Fructus Capsici sauce Need the most bright-coloured color and luster, to win attraction；On the other hand it is the detection technique existing defects of azopigment, it is difficult to find to add The unknown pigment added.
2, the detection present situation of azopigment
The detection of azopigment at present mainly uses liquid chromatography and LC/MS.Most liquid chromatograph Method is the quantitative detecting method for one or more pigments；Liquid chromatography-mass spectrography method comprises two types, and one is to adopt By the mass spectrographic qualitative and quantitative analysis method for one or more pigments of liquid chromatography-tandem quadrupole rod；Another kind is to use The screening method that flight time or track trap high resolution mass spectrum and liquid chromatograph combination set up.These detection methods be primarily present with Lower shortcoming and problem:
1) liquid chromatography and the liquid chromatography-quadrupote mass spectrometry of detection by quantitative can only be examined for known pigment Survey.For disabling pigment, Producer will not express the pigment of use in its product packaging, and therefore this type of detection method does not has Targetedly, it is impossible to determine detection object, it is impossible to meet the detection demand of azopigment in Fructus Capsici sauce.Such as GB/T 5009.35-2003 " mensuration of synthetic coloring matter in food ", GB/T 19681-2005 " the detection side of Detection of Magdala in Food Through dyestuff Method high performance liquid chromatography " etc. standard, be both for the quantitative detecting method of specific pigment, it is impossible to carry out for unknown pigment Detection.
2) based on detection method associated with high resolution mass spectrum-liquid chromatograph, examination can be carried out for azopigment, but On the one hand need the pigment standard substance that user purchasing price is expensive, study and set up the mass spectrometric data storehouse of azopigment, The examination in the range of data base can be realized；On the other hand high resolution mass spectrum is expensive, requires the highest, greatly to operator's technology Most detection units are difficult to.
Summary of the invention
It is an object of the invention to provide one to need not set up pigment standard substance data base, it is possible to realize the same of the unknown Class azopigment detection non-directional screening method.Liquid chromatograph-string that the present invention is relatively low based on price, range is wider The azopigment screening method that connection quadrupole mass spectrometer is set up, thus effectively solve the complete detection of azopigment in Fructus Capsici sauce With a system examination difficult problem, increase substantially detection efficiency, reduce cost and the technology requirement to testing staff.
Technical scheme
The non-directional screening method of azopigment in a kind of Fructus Capsici sauce, comprises the following steps:
(1) adding trifluoroacetic acid aqueous solution in Fructus Capsici sauce and carry out supersound extraction, be subsequently adding saturated nacl aqueous solution, layering (stands Or be allowed to be layered after centrifugal) after take upper liquid to add mass concentration be the formic acid solution of 0.1%, then with 0.22 μm organic facies micropore Membrane filtration, obtains sample；
(2) sample liquid chromatograph-quadrupole mass spectrometer with electron spray ionisation source detects；
(3) if chromatographic peak occurs in the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained, then examination is described Containing azopigment in sample；The precursor scans mass spectrum of each chromatographic peak is extracted the most further one by one from total ion current figure, with Obtain corresponding parent ion mass number；The mass number comparison of the parent ion mass number of acquisition with known azo pigment i.e. be can confirm that The kind of contained azopigment in sample；
If the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained does not has obvious chromatographic peak, then illustrate Sample does not contains azopigment；
Liquid chromatograph parameter:
A) chromatographic column: 100 × 2.1mm, ACQUITY UPLCTMBEH C18,1.7 m(fix phase C18)；
B) flowing phase: A phase: acetonitrile；B phase: mass concentration is 0.1% aqueous formic acid；Column temperature: 40 DEG C；Sample size: 5 L；Flowing Phase gradient is shown in Table 1；
Table 1 condition of gradient elution
；
Mass spectrum operation condition:
A) ion source: electric spray ion source, cation；
B) scan mode: precursor ion-scan is monitored, and precursor ion-scan scope 160amu ~ 600amu, daughter ion mass-to-charge ratio is 156.0；
C) ionization voltage: 3.2kV；Taper hole voltage: 35v；Collision energy 40 ev；
D) ion source temperature: 110 DEG C；Atomization temperature: 400 DEG C；Taper hole gas velocity: 50L/h；Atomization gas flow velocity: 600L/h；Collision Gas: argon；Collision cell pressure: 3.6 × 10-3 mPa。
Above-mentioned non-directional screening method, the extracting method of step (1) is to develop, according to its other party for this examination technology Method can cause that extraction efficiency is undesirable, screening efficiency is greatly reduced.
Above-mentioned non-directional screening method, in step 1,
Fructus Capsici sauce is 1g:5mL with the usage ratio of trifluoroacetic acid aqueous solution, and the condition of supersound extraction is to shake in 40 DEG C of water-baths；
Saturated nacl aqueous solution volume used is equal to the volume of trifluoroacetic acid aqueous solution；
The volume of upper liquid is equal to the volume of formic acid solution.
Aforesaid operations can make Fructus Capsici sauce rapid dispersion in acetonitrile solution, it is achieved the optimum extraction efficiency of azopigment, Isopyknic saturated nacl aqueous solution can realize good distribution with acetonitrile extraction liquid, removes chaff interference to greatest extent.
After azopigment in Fructus Capsici sauce uses acetonitrile extraction, distribute with saturated nacl aqueous solution, in the acetonitrile solution of upper strata After adding isopyknic 0.1% formic acid solution dilution, filtration, inverted liquid-phase chromatographic column separates, and re-uses series connection quadrupole rod matter Spectrum, with m/z156 as daughter ion, carries out precursor ion-scan detection, by the precursor ion of chromatographic peak corresponding in mass chromatogram Mass-to-charge ratio carries out the examination of azopigment.If obtaining the total ion current figure with daughter ion 156, then containing azo in explanation sample Pigment；And check the parent ion mass number corresponding to the chromatographic peak in total ion current figure one by one, compare possible azopigment List, gets final product the disabling contained in confirmatory sample or limits the use of pigment.If parent ion mass number corresponding to a certain chromatographic peak be not In the range of the azopigment known, then may make an addition to the non-food coloring in food for certain the most not yet discovery, can be by literary composition Offer retrieval and test its structure of confirmation further.
The major technique innovation of the present invention
(1) method has powerful disabling, limits the use of pigment ability of discovery
The method applied in the present invention is different from the detection method that current liquid chromatography-tandem quadrupole rod mass spectrum is conventional: square at present Method all uses the pattern of " multiple-reaction monitoring ", i.e. selectes parent ion at series connection quadrupole rod mass spectrographic first order quadrupole rod, through collision Room cracks, then the daughter ion fixed by the monitoring of third level quadrupole rod, real by this ion pair of monitoring " parent-daughter ion " The purpose of existing qualitative and quantitative detection, this pattern is only used for the oriented detection for single compound.The present invention sends out after deliberation Now a lot of azopigments all can produce the fragments characteristic ion that mass-to-charge ratio is 156, have developed precursor scans on this basis Examination pattern, i.e. first order quadrupole rod use scanning pattern, monitoring mass number between 160amu ~ 600amu all from Son, after collision cell cracks, is the daughter ion of 156 in third level quadrupole rod stationary monitoring mass-to-charge ratio, and records and can produce correspondence The mass number of " parent ion " of daughter ion, this parent ion is the target component of examination.Therefore the present invention solves and once finds The disabling of homogeneous structure and the problem limiting the use of azopigment.
(2) need not disabling and limit the use of standard substance and the specialized database comparison of pigment
The present invention is based entirely on the structural information of azopigment, via the common reverse examination parent ion of fragment ion 156, thus Qualitative disabling and the azopigment limited the use of, detection time in need not standard substance comparison, it is not required that built by standard substance Vertical specialty examination data base, testing cost is greatly reduced, and method is not the most lacked standard substance in any laboratory applications, do not has The conditions such as specialized database limit.
(3) examination speed is fast
Inventive samples pre-treatment only needs 20min(supersound extraction 10min+ concussion extraction 2min+ centrifugal layering 3min+ transfer, dilute Release, time-consuming 2min between filter 23 min+ operating procedure), Instrumental Analysis 15min, simple sample non-directional examination overall process only needs 35min.If the examination simultaneously of multiple samples, because pre-treatment is carried out simultaneously, the time also can significantly shorten.Due to this method data analysis Process is simple, and all of suspicious composition all can intuitively manifest in total ion current figure, and the screening method of other high resolution mass spectrums It is required to use complicated software and data base to carry out data process.In general, the method examination speed of the present invention is the fastest Fast, effectively.
(4) instrument popularity is high, and method is workable
The present invention uses liquid chromatography-tandem quadrupole mass spectrometer to carry out non-directional examination, and this instrument is in all mass spectrometers The product that market share is the highest, food safety detection laboratory popularity is the highest the most at home, and experimenter is basic Can skilled operation, the application of this method has stronger operability.And other examination technology all use liquid chromatograph-quadrupole The high-resolution mass spectrometers such as bar/flight time mass spectrum or liquid chromatograph-quadrupole rod/Orbitrap mass spectrometer, the most expensive, in state Interior only minority laboratory above the provincial level has this quasi-instrument, and requires the highest to operator, to the unknown disabling pigment Examination also needs to coordinate complete data base and stronger interpretation of mass spectra ability just can carry out.In general, the grasping of the present invention The property made is higher.
Beneficial effects of the present invention
1, determine the Fructus Capsici sauce 52 batches of different brands, wherein three batches detect Sudan hong Ⅰ, wherein 1 batch of detection para red. Being found that the azopigment of a kind of the unknown in a collection of SUANRONG LAJIANG, its parent ion is 308, through retrieval further, identifies, this thing Matter is industry pigment toluidine red.Application result fully shows, the present invention has for the examination disabling and limiting the use of azopigment Efficiently, the feature such as accurately.
2, the examination of above-mentioned whole 52 batches of Fructus Capsici sauce, was fully completed in 20 hours, has fully demonstrated the present invention the simplest Just advantage.
3, complete the examination of a sample only to need to use 14mL acetonitrile (wherein 10mL is used for sample extraction, and 4mL is flowing Phase), 4g sodium chloride and and the formic acid of trace, reagent cost is less than 2 yuan.If the consumption of use additive method, only standard substance At least more than 50 yuan.The present invention has significant cost advantage.
4, liquid chromatography-tandem quadrupole mass spectrometer used by the present invention, most domestic food inspection laboratory all has joins Standby, the reviewer being typically familiar with chromatographic mass spectrometry is the most operable.This method can be general on the instrument of different brands, and instrument is not Need, through special operationals such as complicated calibration, tunings, compared with high resolution mass spectrum examination, there is higher operability.
5, the inventive method data process short and sweet, can intuitively find can to compare with composition on total ion current figure The chemical formula of azopigment and molecular weight can quickly determine examination object.
6, due to the present invention have simplicity, quickly, economy, instrument hardware require low, the most not by operator's technical merit The features such as restriction, with the obvious advantage in the non-directional examination technology disabling and limiting the use of azopigment, there are good popularization and application Prospect.
Accompanying drawing explanation
Fig. 1 is the total ion current figure that embodiment 1 obtains；
Fig. 2 is precursor ion-scan mass spectrum that the total ion current figure from embodiment 1 extracts, that be defined as the Sudan I；
Fig. 3 is precursor ion-scan mass spectrum that the total ion current figure from embodiment 1 extracts, that be defined as the Sudan II；
Fig. 4 is precursor ion-scan mass spectrum that the total ion current figure from embodiment 1 extracts, that be defined as soudan III；
Fig. 5 is precursor ion-scan mass spectrum that the total ion current figure from embodiment 1 extracts, that be defined as Sudan IV.
Detailed description of the invention
Embodiment 1
1, sample pre-treatments
Weigh 2.0g size-reduced, mixing after Fructus Capsici sauce sample, be placed in 50mL tool plug centrifuge tube in, add 10mL chromatographically pure second Nitrile, concussion, supersound extraction 10min in 40 DEG C of water-baths.Add 10mL saturated nacl aqueous solution after taking-up, firmly shake 2min, quiet Put or centrifugal layering.Take upper strata acetonitrile solution 0.5mL, be placed in 2.5mL centrifuge tube, add 0.5mL0.1% formic acid solution, mixed Even.Through 0.22 μm organic facies filtering with microporous membrane, gained filtrate is sample.
2, instrument and operating condition
2.1 instruments: liquid chromatography-tandem quadrupole mass spectrometer, with electron spray ionisation source.
2.2 liquid chromatograph parameters:
A) chromatographic column: ACQUITY UPLCTMBEH C18(100 × 2.1mm, 1.7 m)；
B) flowing phase: A phase: acetonitrile；B phase: 0.1% aqueous formic acid；Column temperature: 40 DEG C；Sample size: 5 L；Eluent gradient is shown in Table 1:
Table 1 condition of gradient elution
；
2.3 mass spectrum operation conditions
A) ion source: electric spray ion source, cation；
B) scan mode: precursor ion-scan is monitored, precursor ion-scan scope 160amu-600amu；Daughter ion mass-to-charge ratio 156.0amu；
C) ionization voltage: 3.2kV；Taper hole voltage: 35v；Collision energy 40 ev；
D) ion source temperature: 120 DEG C；Atomization temperature: 500 DEG C；Taper hole gas velocity: 150L/h；Atomization gas flow velocity: 800L/h；Touch Hit gas: argon, collision cell pressure: 3.6 × 10-3 mPa。
3, the analysis of screening results
Criterion: substantially can distinguish if existing in the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained Chromatographic peak, then containing azopigment in explanation sample；Extract one by one from total ion current figure the most further the mother of each chromatographic peak from Son scanning mass spectrum, to obtain corresponding parent ion mass number；By the parent ion mass number obtained and the matter of known azo pigment Amount number comparison i.e. can confirm that the kind of contained azopigment in sample；If parent ion mass number corresponding to a certain chromatographic peak be not In the range of the azopigment known, then may make an addition to the non-food coloring in food for certain the most not yet discovery, can be by literary composition Offer retrieval and test its structure of confirmation further.If the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained In there is no an obvious chromatographic peak, then explanation sample does not contains azopigment.
If Fig. 1 is that examination obtains and has the total ion current figure of obvious chromatographic peak, illustrate in testing sample containing azo color Element.Extract the precursor ion-scan mass spectrum (Fig. 2-Fig. 4) of each chromatographic peak the most one by one, check corresponding parent ion quality Number, compares possible azopigment chemical constitution, confirms in sample containing the Sudan I, the Sudan II, soudan III and Sudan IV.
Embodiment 2
Using the Fructus Capsici sauce 52 batches of different brands as sample to be tested, use the operation of embodiment 1, wherein three batches detect the Sudan Red No. 1, wherein 1 batch of detection para red.Being found that the azopigment of a kind of the unknown in a collection of SUANRONG LAJIANG, its parent ion is 308, through retrieval further, to identify, this material is industry pigment toluidines.

Claims (2)

1. the non-directional screening method of azopigment in a Fructus Capsici sauce, it is characterised in that comprise the following steps:
(1) in Fructus Capsici sauce, add trifluoroacetic acid aqueous solution and carry out supersound extraction, be subsequently adding saturated nacl aqueous solution, take after layering It is the formic acid solution of 0.1% that layer liquid adds mass concentration, then with 0.22 μm organic facies filtering with microporous membrane, obtains sample；
(2) sample liquid chromatograph-quadrupole mass spectrometer with electron spray ionisation source detects；
(3) if chromatographic peak occurs in the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained, then examination is described Containing azopigment in sample；The precursor scans mass spectrum of each chromatographic peak is extracted the most further one by one from total ion current figure weight, with Obtain corresponding parent ion mass number；The mass number comparison of the parent ion mass number of acquisition with known azo pigment i.e. be can confirm that The kind of contained azopigment in sample；
If the precursor ion-scan total ion current figure with m/z156 as daughter ion obtained does not has obvious chromatographic peak, then illustrate Sample does not contains azopigment；
Liquid chromatograph parameter:
Chromatographic column: 100 × 2.1mm, fixing phase C18,1.7 m；
Flowing phase: A phase: acetonitrile；B phase: mass concentration is 0.1% aqueous formic acid；Column temperature: 40 DEG C；Sample size: 5 L；Flowing phase Gradient is shown in Table 1；
Table 1
；
Mass spectrum operation condition:
A) ion source: electric spray ion source, cation；
B) scan mode: precursor ion-scan is monitored, and precursor ion-scan scope 160amu-600amu, daughter ion mass-to-charge ratio is 156.0；
C) ionization voltage: 3.2kV；Taper hole voltage: 35v；Collision energy 40 ev；
D) ion source temperature: 110 DEG C；Atomization temperature: 400 DEG C；Taper hole gas velocity: 50L/h；Atomization gas flow velocity: 600L/h；Collision Gas: argon；Collision cell pressure: 3.6 × 10-3 mPa。
Non-directional screening method the most according to claim 1, it is characterised in that in step 1,
Fructus Capsici sauce is 1g:5mL with the usage ratio of trifluoroacetic acid aqueous solution, and the condition of supersound extraction is to shake in 40 DEG C of water-baths；
Saturated nacl aqueous solution volume used is equal to the volume of trifluoroacetic acid aqueous solution；
The volume of upper liquid is equal to the volume of formic acid solution.
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